CN112842924B - High-viscosity moisturizing amino acid facial cleanser embedded with squalane as well as preparation method and application of facial cleanser - Google Patents
High-viscosity moisturizing amino acid facial cleanser embedded with squalane as well as preparation method and application of facial cleanser Download PDFInfo
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Abstract
The invention provides squalane-embedded high-viscosity moisturizing amino acid facial cleanser and a preparation method and application thereof, wherein the raw materials of the facial cleanser comprise: glycerol, butylene glycol, potassium cocoyl glycinate, sodium cocoyl malate, alkyl glycoside, cocamidopropyl betaine, cetostearyl alcohol, ethylene glycol stearate, citric acid, glyceryl stearate, collagen, squalane liposome, disodium edetate, p-hydroxyacetophenone, vitamin E acetate and water. The invention also provides a preparation method of the squalane liposome. According to the invention, through increasing the amino acid surface active aggregation groups, the squalane-embedded high-viscosity moisturizing amino acid facial cleanser solves the problems of high dosage and difficult thickening of amino acid surface living body products, so that the temperature, viscosity and mildness of the facial cleanser are greatly improved in the cleaning effect on skin dirt and the moisturizing degree after use; meanwhile, the surface activity dosage of the facial cleanser and the usage amount of the product in use are reduced.
Description
Technical Field
The invention belongs to the technical field of cosmetic production, and particularly relates to squalane-embedded high-viscosity moisturizing amino acid facial cleanser as well as a preparation method and application thereof.
Background
With the updating of the cosmetic formula framework, the requirements of people on the cosmetic quality are improved, and daily chemical products emerge endlessly. At present, the facial cleansing products in China are various in types, and it is not difficult to find that in over 200 million of the cosmetics already put on record, the main cleansing products for the face mainly comprise facial cleanser, and the facial cleanser products on the market comprise soap base, anionic activator and amphoteric surfactant as main agents, so that the surfactant has abundant foam, strong detergency contrast, large degreasing property, and particularly has strong feeling after use due to large irritation of the soap base, and a large amount of thickening agent and auxiliary surfactant need to be added into the formula of the amino acid facial cleanser. The original safe and mild properties of the amino acid surfactant are destroyed by the formula structure.
The amino acid facial cleanser with amino acid as main surface activity has small micelle particle size, high critical micelle concentration and extremely difficult thickening, and the amino acid facial cleanser in the market is a thickening agent which basically increases the dosage of amino acid surfactant and assists various macromolecules and various thickening agents to increase the viscosity and stability of products. However, the price of amino acid surfactants is more expensive than soap base and anionic surfactants. This results in higher cost of amino acid facial cleanser and difficult mass production of the formula of the product.
Such as: CN106726698A discloses an amino acid type facial cleanser and a preparation method thereof, and the amino acid type facial cleanser comprises: 0-30 wt% of amino acid surfactant, 1-15 wt% of non-amino acid surfactant, 0.5-2 wt% of thickener, 5-30 wt% of humectant, 0.2-2.5 wt% of neutralizer, 0.1-1 wt% of conditioner and deionized water, which are neutral, mild, skin-friendly, safe and non-irritant, and can deeply clean skin, the thickening into paste is realized mainly by adding high content of amino acid surfactant, non-amino acid surfactant and 0.5-2 wt% of thickener, the manufacturing cost is higher, the degreasing force is higher, and the water-deficient tight feeling after skin cleaning can be brought. When used, the facial cleanser containing substantially all amino acid surfactants on the market is difficult to overcome the skin feeling of pseudo-smooth oily film feeling caused by long-time washing of the amino acid surfactants.
Disclosure of Invention
The invention aims to provide a squalane-embedded high-viscosity moisturizing amino acid facial cleanser as well as a preparation method and application thereof, solves the problem that a thickening agent is used for increasing the viscosity of the facial cleanser with amino acid as a main surfactant in the prior art, reduces/avoids the addition of a non-amino acid surfactant for an apparent living system, and has safety and mildness.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides squalane-embedded high-viscosity moisturizing amino acid facial cleanser, which comprises the following components in parts by weight:
the invention also provides a preparation method of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser, which comprises the following steps:
(1) Adding the first part of the glycerol, the butanediol, the potassium cocoyl glycinate, the sodium cocoyl malic amino acid, the alkyl glycoside, the cocamidopropyl betaine, the cetostearyl alcohol, the ethylene glycol stearate, the glyceryl stearate, the disodium ethylene diamine tetraacetate, the vitamin E acetate, the p-hydroxyacetophenone and the deionized water with the above dosage, vacuumizing, heating and stirring for reaction to obtain a phase A;
(2) Adding citric acid into the second part of the deionized water, and stirring and dissolving to obtain a citric acid aqueous solution as a phase B;
(3) Adding collagen into the third part of the deionized water, and stirring and dissolving to obtain a phase C;
(4) Adding the phase B obtained in the step (2) into the phase A obtained in the step (1), heating, stirring, cooling and obtaining a phase D;
(5) Adding the C phase obtained in the step (3) into the D phase obtained in the step (4), keeping the temperature, stirring, cooling and obtaining an E phase;
(6) And (3) adding the squalane liposome into the phase E obtained in the step (5), keeping the temperature, stirring, cooling, standing and aging to obtain the squalane-embedded high-viscosity moisturizing amino acid facial cleanser.
Further: the squalane liposome is prepared by a method a or a method b:
method a, (a 1): after the emulsification kettle is cleaned and disinfected, adding 20-28 parts of squalane, 3-8 parts of caprylic/capric triglyceride and 5-6 parts of phytosterol into the emulsification kettle, heating, stirring, cooling and discharging to a raw material barrel;
(a2) The method comprises the following steps Placing the raw material barrel in the step (a 1) in a refrigerator for cooling and storing, taking out, heating and preserving, cooling and storing again, and performing cold-hot alternating circulation for 3-6 periods for later use;
(a3) The method comprises the following steps After the emulsification kettle is cleaned and disinfected, 8-12 parts of deionized water are added, 10-15 parts of hydrogenated lecithin are added into the emulsification kettle, sealed stirring is started, and nitrogen is introduced and stirred;
(a4) The method comprises the following steps Adding the raw materials treated in the step (a 2) into the emulsifying kettle in the step (a 3), vacuumizing, stirring, heating and preserving heat; adding 3 parts of 1,2-hexanediol and deionized water, vacuumizing the emulsifying kettle, increasing the stirring speed, opening the homogenizing shear for 8-12 min, reducing the stirring speed, cooling and discharging to obtain the squalane liposome;
or method b, (b 1): after the emulsification kettle is cleaned and disinfected, 8-12 parts of deionized water are added, 10-15 parts of hydrogenated lecithin are added into the emulsification kettle, sealed stirring is started, and nitrogen is introduced and stirred;
(b2) The method comprises the following steps Adding 20-28 parts of squalane, 3-8 parts of caprylic/capric triglyceride and 5-6 parts of phytosterol into an emulsifying kettle, vacuumizing, stirring, heating and preserving heat; and adding 3 parts of 1,2-hexanediol and deionized water, increasing the stirring speed, opening the homogenizing shear for 8-12 min, reducing the stirring speed, and cooling and discharging to obtain the squalane liposome.
Further, the reaction temperature of the step (1) is 71-80 ℃, and the stirring rotation speed is 300-500 rpm.
Further, the temperature rise temperature of the step (4) is 76-85 ℃, and the temperature drop temperature is 56-65 ℃; the stirring speed is 300-500 rpm.
Further, the weight of the first part of deionized water, the weight of the second part of deionized water and the weight of the third part of deionized water are respectively 60-90%, 5-20% and 5-20% of the total weight of deionized water.
Further, the temperature reduction temperature in the step (5) is 36-45 ℃; the stirring speed is 300-500 rpm.
Further, the cooling speed in the cooling in the steps (4) and (5) is 0.5-1.5 ℃/min.
Further, the total amount of the deionized water in the steps (a 3) and (a 4) is 20-28 parts; the total amount of the deionized water in the steps (b 1) and (b 2) is 20-28 parts.
Further, the air pressure for vacuumizing in the step (1) is below-0.05 MP.
Further, the B phase, the C phase and the squalane liposome in the steps (4) to (6) are added dropwise at a speed of 50 to 100ml/min.
Further, the stirring time in the step (1) is 26-35 min; the stirring time of the step (4) is 26-35 min; the stirring time in the step (5) is 16-55 min; the stirring time of the step (6) is 16-25 min.
Further, in the step (a 1), the temperature is increased to 58-65 ℃, the temperature is decreased to room temperature, and the stirring time is 18-25 min.
Further, in the step (a 2), the temperature is reduced to be below 0 ℃, the temperature is increased to be between 21 and 30 ℃, the temperature-reducing preservation time is between 16 and 50 hours, and the temperature-increasing preservation time is between 16 and 50 hours.
Further, in the steps (a 3) and (b 1), the nitrogen gas is introduced for 3-6 min, the stirring speed is 200-300 rpm, and the stirring time is 6-12 min.
Further, in the step (a 4), the stirring speed is 200-300 rpm, the temperature rise and preservation temperature is 70-75 ℃, and the preservation time is 18-25 minutes; the stirring speed is increased to 400-500 rpm, and the stirring speed is reduced to 150-200 rpm.
The invention also provides application of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser in preparation of cosmetics.
Compared with the prior art, the invention has the advantages and beneficial effects that:
the invention has low cost, simple production and no thickener, and is suitable for mass production. The invention is prepared by raw materials such as squalane liposome, deionized water and the like. The invention is extremely mild, without thickener addition, but can have extremely high viscosity. Can protect and supplement skin barrier, is easy to clean, has no special pseudo-slippery feeling of common amino acid surfactant, and has long water locking time. All the raw materials have good biodegradability and are environment-friendly.
The people who select the product with the amino acid framework formula mainly have sensitive skin and sensitive skin consumers. The amino acid facial cleanser disclosed by the invention is extremely high in mildness, and does not have the characteristic that the surfactant product in an amino acid surfactant facial cleanser system is high in dosage or needs to be added with a large amount of thickening agent to realize thickening, so that the mildness, viscosity and mildness of the facial cleanser can greatly improve the cleaning effect on skin dirt and the moisture retention after use.
The facial cleanser disclosed by the invention is free of the addition of the thickening agent, the particle size of the amino acid surface active aggregation group micelle is increased for thickening, the liposome microcapsule formed after the squalane double-layer wrapping is embedded in the gap of the increased amino acid surface active micelle group, and the squalane is subjected to denaturation treatment, so that the dissipation of squalane is increased, and the liposome microsphere can quickly achieve a good skin nourishing effect, so that the irritation of the facial cleanser to the skin is greatly reduced. The skin permeability is increased by the squalane encapsulated by the microcapsules, and the skin barrier can be supplemented, protected and repaired. The low-irritation alkyl glycoside, the cocamidopropyl betaine and the amino acid are compounded in the formula, so that the foaming degree can be increased, the skin cleaning use feeling can be improved, and the surface activity use amount of the facial cleanser system and the use amount of the product in use are reduced. Meanwhile, the invention carries out denaturation treatment on squalane, and can quickly achieve good skin nourishing effect by utilizing liposome microspheres through improving the dissipation performance of the squalane after the denaturation treatment.
Detailed Description
The following embodiments better illustrate the present invention. However, the present invention is not limited to the following examples.
The squalane-embedded high-viscosity moisturizing amino acid facial cleanser comprises the following components in parts by weight:
the raw materials for embedding the squalane liposome structure are as follows according to parts by weight:
according to the formula disclosed by the invention, no thickening agent is added, and the system thickening is carried out by increasing the micelle particle size of the potassium cocoyl glycinate and the sodium cocoyl malate. The liposome microcapsule formed after the squalane double-layer coating is embedded between the enlarged gaps of the amino acid surface active micelle groups of the potassium cocoyl glycinate and the sodium cocoyl malate. Can reduce the stimulation brought by the surfactant, and simultaneously can ensure that the coated squalane quickly permeates skin, supplements and repairs skin barriers and achieves the effect of lasting moisture preservation.
Example 1: two preparation methods of squalane liposome
1. The preparation method a of the squalane liposome comprises the following steps:
1. after a 100L pilot-scale emulsification kettle (hereinafter referred to as an emulsification kettle) is cleaned and disinfected, adding 28 parts of squalane, 8 parts of caprylic/capric triglyceride and 5 parts of phytosterol into the emulsification kettle, stirring at 200-300 rpm, heating to 60 ℃, stirring for 20min, cooling, naturally cooling to room temperature, and discharging to a raw material barrel.
2. Placing the raw material barrel in the step 1 in a refrigerator, cooling to-5 ℃, preserving for 48h, taking out, heating to 25 ℃, and preserving heat for 48h; after the heat preservation is finished, the mixture is put into a refrigerator to be cooled to-5 ℃ and stored for 48 hours, and the cold and hot alternate circulation is carried out for 5 periods for standby.
3. After the emulsification kettle is cleaned and disinfected, 10 parts of deionized water is added, 12 parts of hydrogenated lecithin is added into the emulsification kettle, stirring is started by inching, valves of the emulsification kettle are closed, nitrogen is introduced for 5min, and the rotation speed is controlled to be 200-300 rpm and kept for 10min.
4. Adding the raw materials treated in the step 2 into the emulsifying kettle in the step 3 through an oil phase pot, vacuumizing to below-0.05 MP, controlling the rotating speed to be 200-300 rpm, heating to 70-75 ℃, and preserving heat for 20 minutes; adding 1,2-hexanediol and the rest deionized water into a water phase pot, vacuumizing the emulsifying kettle to below-0.05 MP, keeping the temperature at 70-75 ℃, increasing the stirring speed to 400-500 rpm, opening the homogenizing shear, controlling the homogenizing shear speed to 20000rpm, and keeping for 10min. Reducing the stirring speed, controlling the rotating speed to be 150-200 rpm, cooling to 40 ℃, controlling the cooling speed to be 1 ℃/min and 40 ℃, introducing nitrogen to discharge after evacuation, and obtaining the squalane liposome.
2. The preparation method b of the squalane liposome comprises the following steps:
1. after the emulsification kettle is cleaned and disinfected, 10 parts of deionized water is added, 12 parts of hydrogenated lecithin is added into the emulsification kettle, stirring is started by inching, valves of the emulsification kettle are closed, nitrogen is introduced for 5min, and the rotation speed is controlled to be 200-300 rpm and kept for 10min.
2. Adding 28 parts of squalane, 8 parts of caprylic/capric triglyceride and 5 parts of phytosterol into an emulsifying kettle through an oil phase pot, vacuumizing to be below-0.05 MP, controlling the rotating speed to be 200-300 rpm, heating to 70-75 ℃, and preserving heat for 20 minutes; adding 1,2-hexanediol and the rest deionized water into an aqueous phase pot, vacuumizing an emulsifying kettle to below-0.05 MP, keeping the temperature at 70-75 ℃, increasing the stirring speed to 400-500 rpm, opening the homogeneous shearing, controlling the homogeneous shearing speed to 20000rpm, keeping the stirring speed for 10min, reducing the stirring speed, controlling the rotating speed to 150-200 rpm, reducing the temperature to 40 ℃, controlling the cooling speed to 1 ℃/min,40 ℃, introducing nitrogen, evacuating and discharging to obtain the undenatured squalane liposome.
Example 2: preparation of squalane-embedded high-viscosity moisturizing amino acid facial cleanser
The preparation method of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser comprises the following steps of:
1. adding 90% of the total weight of glycerol, butanediol, potassium cocoyl glycinate, sodium cocoyl malate, alkyl glycoside, cocamidopropyl betaine, cetostearyl alcohol, glyceryl stearate, p-hydroxyacetophenone, ethylene glycol stearate, disodium ethylene diamine tetraacetate, vitamin E acetate and deionized water into a 150L pilot scale reaction kettle (hereinafter referred to as a reaction kettle) in sequence, stirring by inching, adjusting the revolution to 300rpm, heating to 75 ℃, vacuumizing to-0.05 MP, and stirring for 30min to obtain a phase A.
2. Adding citric acid into 5% of deionized water, stirring to obtain citric acid aqueous solution, and getting phase B.
3. Adding collagen into the rest 5% of deionized water, stirring and dissolving to obtain protein dispersed colloid phase C.
4. And (3) dropwise adding the phase B obtained in the step (2) into the phase A obtained in the step (1) at a rate of 50ml/min, controlling the temperature to be increased to 80 ℃ after the dropwise adding is finished, stirring at a speed of 500rpm, keeping the pressure in the reaction kettle to be less than-0.05 MP, cooling to 60 ℃ by introducing cooling water after the temperature is kept for 30min, and controlling the cooling speed to be 1 ℃/min to obtain a phase D.
5. And (3) dropwise adding the phase C obtained in the step (3) into the phase D obtained in the step (4) at a speed of 100ml/min, controlling the temperature to be 60 ℃ after dropwise adding, rotating at a speed of 500rpm, controlling the pressure in the reaction kettle to be less than-0.05 MP, stirring for 20min, cooling to 40 ℃ by introducing cooling water, and controlling the cooling speed to be 0.5 ℃/min to obtain the phase E (rotating at a speed of 300rpm after cooling to 50 ℃).
6. And (3) dropwise adding the squalane liposome into the phase E obtained in the step (5) at a rate of 100ml/min, controlling the temperature to be 40 ℃ after the dropwise adding is finished, controlling the revolution to be 300rpm, controlling the pressure in the reaction kettle to be less than-0.05 MP, stirring for 20min, cooling to room temperature, discharging, standing at room temperature, aging for 24 hours, and obtaining the squalane-embedded high-viscosity moisturizing amino acid facial cleanser which is a qualified finished product.
Example 3: testing of squalane-embedded high viscosity moisturizing amino acid facial cleanser
1. Formulation of
The raw material formula and the weight parts of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser are shown in table 1;
table 1 formula of amino acid facial cleanser of the present invention
| Formulation A | Formulation B | Formulation C | Formulation D | |
| Glycerol | 40 portions of | 35 portions of | 30 portions of | 25 portions of |
| Butanediol | 5 portions of | 5 portions of | 8 portions of | 8 portions of |
| Coconut oil acyl potassium glycinate | 14 portions of | 12 portions of | 10 portions of | 8 portions of |
| Sodium cocoyl malate | 4 portions of | 4 portions of | 6 portions of | 2 portions of |
| Alkyl glycosides | 10 portions of | 8 portions of | 6 portions of | 5 portions of |
| Cocoamidopropyl betaine | 5 portions of | 5 portions of | 5 portions of | 8 portions of |
| Cetostearyl alcohol | 2 portions of | 2 portions of | 1 part of | 1 part of |
| Ethylene glycol stearate | 4 portions of | 4 portions of | 2 portions of | 1.5 parts of |
| Citric acid | 2 portions of | 2 portions of | 1.5 parts of | 1.5 parts of |
| Glycerol stearate | 1 part of | 1 part of | 0.5 portion | 0.5 part of |
| Collagen protein | 1 part of | 1 part of | 1 part of | 0.5 portion |
| Squalane liposome | 8 portions of | 6 portions of | 6 portions of | 4 portions of |
| Ethylenediaminetetraacetic acid disodium salt | 0.05 part | 0.05 part | 0.05 part of | 0.1 part |
| P-hydroxyacetophenone | 0.5 portion | 0.5 portion | 0.5 part of | 0.5 portion |
| Vitamin E acetate | 1 part of | 1 part of | 1 part of | 1 part of |
| Deionized water | 22.45 portions of | 33.45 parts | 41.45 parts | 53.4 parts |
| Is totaled | 120 portions of | 120 portions of | 120 portions of | 120 portions of |
The raw material formula and the parts by weight of the squalane liposome are shown in table 2;
TABLE 2 formulation of squalane liposomes of the present invention
The raw materials used in the present invention are all commercially available.
2. Preparation method
1. Squalane liposome prepared according to the preparation method described in example 1, formulation E in example 3; sampling, selecting emulsified particles with different sizes by microscopic image control analysis under a high power microscope, and measuring the particle diameter by a three-point method, wherein the measured particle diameter is 10 nm-50 nm squalane liposome.
2. The facial cleanser was prepared according to the preparation method described in example 3, and the formula was formula a in example 3.
(1) The obtained facial cleanser is high-viscosity moisturizing amino acid facial cleanser embedded with squalane, and the viscosity of the facial cleanser is tested after the facial cleanser is stood and aged for 24 hours at room temperature;
the NDJ-1 type rotary viscometer is selected to test conditions: rotor No. 4, 12rpm;
41 (index reading) × 500 (coefficient) =20500mpa.s.
(2) And (3) performing foam test after the squalane-embedded high-viscosity moisturizing amino acid facial cleanser is stood and aged for 24 hours at room temperature, wherein the test method is measured by using a Roche foamer according to GB/17173:
and (3) testing mass concentration: 2 percent;
and (3) testing temperature: 40 ℃;
the initial foam height was: 125 + -3 mm (3 measurements are averaged);
foam height after 10min 116. + -.3 mm (3 measurements are averaged).
(3) Spot-pasting experiment: selecting 31 subjects, wherein the age of the subjects is 23-38 years old;
the number of sensitive muscles is required to be at least 50 percent of the total number (the number of sensitive muscle screening rolls is measured by 5 percent lactic acid solution), and the number of actual sensitive muscles is 17;
applying spots of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser to the curved side of the forearm of a subject, lightly pressing with hands to uniformly apply the patches to the skin for 24 hours, removing the spots, and recording reaction results for 30min, 24 hours and 48 hours after the indentations disappear;
all the testers had negative reaction. No weak erythema, edema, infiltration, pimple, etc.
(4) Moisture content of skin: the skin moisture content is one of main indexes for detecting the moisture retention of a formula and the influence on the skin barrier, and the facial cleanser with an amino acid formula with a large sale amount on the market and the facial cleanser disclosed by the invention are selected for reference; under the constant temperature and constant relative humidity (25 ℃, 35) test conditions of an organoleptic test laboratory, a skin moisture content test probe is used to select 11 human subjects with the ages of 25-38 years from a Cornemeter CM825 (Courage + Khazaka, germany) of Germany to carry out the test, and the test results are shown in the following table 3;
TABLE 3 test results
| Time | Blank space | Commercial facial cleanser | High-viscosity moisturizing amino acid facial cleanser |
| 30min | 27.31±1.97 | 23.15±1.65 | 31.38±3.35 |
| 1h | 27.55±2.18 | 23.19±2.51 | 33.49±3.43 |
| 7h | 28.63±3.31 | 27.89±2.64 | 31.15±2.57 |
The high-viscosity moisturizing amino acid facial cleanser can protect and supplement skin barrier. Under a stable environment, the measured data shows that the water locking and moisture retention time is still higher than a blank value.
Example 4: testing of squalane-embedded high viscosity moisturizing amino acid facial cleanser
1. The preparation method is as described in example 1, and the formulation is formulation E in example 3; sampling, selecting emulsified particles with different sizes by microscopic image control analysis under a high power microscope, and measuring the particle diameter by a three-point method, wherein the measured particle diameter is the squalane liposome with the particle diameter of 30 nm-60 nm.
2. The facial cleanser is prepared according to the preparation method of the example 3, and the formula is the formula A in the example 3;
(1) The obtained facial cleanser is high-viscosity moisturizing amino acid facial cleanser embedded with squalane, and the viscosity of the facial cleanser is tested after the facial cleanser is stood and aged for 24 hours at room temperature;
the NDJ-1 type rotary viscometer is selected to test conditions: rotor No. 4, 12rpm;
40 (index reading) × 500 (coefficient) =20000mpa.s.
(2) And (3) performing foam test after the squalane-embedded high-viscosity moisturizing amino acid facial cleanser is stood and aged for 24 hours at room temperature, wherein the test method is measured by using a Roche foamer according to GB/17173:
and (3) testing mass concentration: 2 percent;
and (3) testing temperature: 40 ℃;
the initial foam height was: 120 + -3 mm (3 measurements are averaged);
after 10min the foam height was 111. + -.3 mm (3 measurements were averaged).
(3) Spot-pasting experiment: selecting 32 testees, wherein the age of the testees is 23-38 years old;
the number of sensitive muscles is required to be at least 50 percent of the total number (the number of sensitive muscle screening rolls is measured by 5 percent lactic acid solution), and the number of actual sensitive muscles is 18;
applying spots of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser to the curved side of the forearm of a subject, lightly pressing with hands to uniformly apply the patches to the skin for 24 hours, removing the spots, and recording reaction results for 30min, 24 hours and 48 hours after the indentations disappear;
all the testers had negative reaction. No weak erythema, edema, infiltration, pimple, etc.
(4) Moisture content of skin: under the constant temperature and constant relative humidity (25 ℃, 35 ℃) test conditions of a sensory test laboratory, 11 human subjects aged 25 to 38 years were selected by a corneometer CM825, a company CK, germany (Courage + Khazaka, germany), using a skin moisture content test probe, and the test results are as shown in table 4 below.
TABLE 4 test results
| Time | Blank space | Commercial facial cleanser | High-viscosity moisturizing amino acid facial cleanser |
| 30min | 27.21±1.75 | 23.06±1.59 | 30.35±2.65 |
| 1h | 27.38±2.05 | 23.03±2.51 | 32.19±3.22 |
| 7h | 28.54±3.28 | 27.88±2.56 | 30.56±2.85 |
The high viscosity moisturizing amino acid facial cleanser can protect and supplement skin barrier. Under a stable environment, the measured data shows that the water locking and moisturizing time is still higher than a blank value.
Example 5: testing of squalane-embedded high viscosity moisturizing amino acid facial cleanser
1. Squalane liposomes were prepared according to the preparation method described in example 1, formulation F in example 3; sampling, selecting emulsified particles with different sizes by microscopic image control analysis under a high power microscope, and measuring the particle diameter by a three-point method, wherein the measured particle diameter is the squalane liposome with the particle diameter of 30 nm-60 nm.
2. The facial cleanser is prepared according to the preparation method of the example 3, and the formula is the formula B in the example 3;
(1) The obtained facial cleanser is high-viscosity moisturizing amino acid facial cleanser embedded with squalane, and the viscosity of the facial cleanser is tested after the facial cleanser is stood and aged for 24 hours at room temperature;
NDJ-1 type rotary viscometer test conditions are selected: rotor No. 3, 6rpm;
84.0 (pointer reading) × 200 (coefficient) =16800mpa.s.
(2) And (3) performing foam test after the squalane-embedded high-viscosity moisturizing amino acid facial cleanser is stood and aged for 24 hours at room temperature, wherein the test method is measured by using a Roche foamer according to GB/17173:
and (3) testing mass concentration: 2 percent;
and (3) testing temperature: at 40 ℃;
the initial foam height was: 118 ± 3mm (3 measurements averaged);
foam height after 10min 114. + -.3 mm (3 measurements mean).
(3) Spot pasting experiment: selecting 33 subjects, wherein the age of the subjects is 23-38 years old;
the number of the sensitive muscles is required to be at least 50 percent of the total number (the sensitive muscle screening test is performed by using a 5 percent lactic acid solution), and the number of the actual sensitive muscles is 19;
applying spot test of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser to the curved side of the forearm of a testee, lightly pressing with hands to uniformly apply the squalane to the skin for 24 hours, removing the spot test, and recording reaction results for 30min, 24 hours and 48 hours after the indentation disappears;
all the subjects were negative. No weak erythema, edema, infiltration, pimple, etc.
(4) Moisture content of skin: under the constant temperature and constant relative humidity (25 ℃, 35) test conditions of an organoleptic test laboratory, a skin moisture content test probe is used to select 9 human subjects with the ages of 25-38 years from a Cornemeter CM825 (Courage + Khazaka, germany) of Germany to carry out the test, and the test results are shown in the following table 5;
TABLE 5 test results
| Time | Blank space | Commercial facial cleanser | High-viscosity moisturizing amino acid facial cleanser |
| 30min | 28.55±1.52 | 24.25±1.18 | 36.38±3.85 |
| 1h | 28.95±2.42 | 25.26±2.91 | 38.72±2.36 |
| 7h | 29.21±3.15 | 27.18±3.25 | 32.50±2.42 |
The high viscosity moisturizing amino acid facial cleanser can protect and supplement skin barrier. Under a stable environment, the measured data shows that the water locking and moisturizing time is still higher than a blank value.
Example 6: testing of squalane-embedded high viscosity moisturizing amino acid facial cleanser
1. Squalane liposomes were prepared according to the preparation method described in example 1, formulation F in example 3; sampling, selecting emulsified particles with different sizes by microscopic image control analysis under a high-power microscope, and measuring the particle size by a three-point method, wherein the measured particle size is 10-50 nm squalane liposome.
2. The facial cleanser is prepared according to the preparation method of the example 3, and the formula is the formula B in the example 3;
(1) The obtained facial cleanser is high-viscosity moisturizing amino acid facial cleanser embedded with squalane, and the viscosity of the facial cleanser is tested after the facial cleanser is stood and aged for 24 hours at room temperature;
the NDJ-1 type rotary viscometer is selected to test conditions: rotor No. 3, 6rpm;
88.0 (pointer reading) × 200 (coefficient) =17600mpa.s.
(2) And (3) performing foam test after the squalane-embedded high-viscosity moisturizing amino acid facial cleanser is stood and aged for 24 hours at room temperature, wherein the test method is measured by using a Roche foamer according to GB/17173:
and (3) testing mass concentration: 2 percent;
and (3) testing temperature: at 40 ℃;
the initial foam height was: 125 + -3 mm (3 measurements are averaged);
foam height after 10min 120. + -.3 mm (average of 3 measurements).
(3) Spot pasting experiment: selecting 33 subjects, wherein the age of the subjects is 23-38 years old;
the number of sensitive muscles is required to be at least 50 percent of the total number (the number of sensitive muscle screening rolls is measured by 5 percent lactic acid solution), and the number of actual sensitive muscles is 19;
applying spot test of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser to the curved side of the forearm of a testee, lightly pressing with hands to uniformly apply the squalane to the skin for 24 hours, removing the spot test, and recording reaction results for 30min, 24 hours and 48 hours after the indentation disappears;
all the testers had negative reaction. No weak erythema, edema, infiltration, pimple, etc.
(4) Moisture content of skin: under the constant temperature and constant relative humidity (25 ℃, 35) test conditions of an organoleptic test laboratory, a skin moisture content test probe is used to select 10 human subjects with the ages of 25-38 years from a Cornemeter CM825 (Courage + Khazaka, germany) of Germany to carry out the test, and the test results are shown in the following table 6;
TABLE 6 test results
| Time | Blank space | Commercial facial cleanser | High-viscosity moisturizing amino acid facial cleanser |
| 30min | 28.05±1.88 | 24.11±1.58 | 37.88±1.65 |
| 1h | 28.40±2.84 | 25.31±2.63 | 39.42±2.62 |
| 7h | 29.21±3.30 | 27.83±3.66 | 33.80±3.48 |
The high viscosity moisturizing amino acid facial cleanser can protect and supplement skin barrier. Under a stable environment, the measured data shows that the water locking and moisturizing time is still higher than a blank value.
Example 7: testing of squalane-embedded high viscosity moisturizing amino acid facial cleanser
1. Squalane liposome prepared according to the preparation method described in example 1, formulation G in example 3; sampling, selecting emulsified particles with different sizes by microscopic image control analysis under a high power microscope, and measuring the particle diameter by a three-point method, wherein the measured particle diameter is 10 nm-50 nm squalane liposome.
2. The facial cleanser was prepared according to the preparation method described in example 3, and the formula was formula C in example 3;
(1) The obtained facial cleanser is high-viscosity moisturizing amino acid facial cleanser embedded with squalane, and the viscosity of the facial cleanser is tested after the facial cleanser is stood and aged for 24 hours at room temperature;
the NDJ-1 type rotary viscometer is selected to test conditions: rotor No. 3, 6rpm;
76.5 (pointer reading) =200 (coefficient) =15300mpa.s.
(2) And (3) performing foam test after the squalane-embedded high-viscosity moisturizing amino acid facial cleanser is stood and aged for 24 hours at room temperature, wherein the test method is measured by using a Roche foamer according to GB/17173:
and (3) testing mass concentration: 2 percent;
and (3) testing temperature: 40 ℃;
the initial foam height was: 133 + -3 mm (3 measurements are averaged);
foam height after 10min 116. + -.3 mm (3 measurements are averaged).
(3) Spot-pasting experiment: selecting 28 subjects, wherein the age of the subjects is 23-35 years;
the number of sensitive muscles is required to be at least 50 percent of the total number (the number of sensitive muscle screening rolls is measured by 5 percent lactic acid solution), and the number of actual sensitive muscles is 17;
applying spots of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser to the curved side of the forearm of a subject, lightly pressing with hands to uniformly apply the patches to the skin for 24 hours, removing the spots, and recording reaction results for 30min, 24 hours and 48 hours after the indentations disappear;
all the testers had negative reaction. No weak erythema, edema, infiltration, pimple, etc.
(4) Moisture content of skin: under the constant temperature and constant relative humidity (25 ℃, 35) test conditions of an organoleptic test laboratory, a skin moisture content test probe is used to select 10 human subjects with the ages of 25-38 years from a Cornemeter CM825 (Courage + Khazaka, germany) of Germany to carry out the test, and the test results are shown in the following table 7;
TABLE 7 test results
| Time | Blank space | Commercial facial cleanser | High-viscosity moisturizing amino acid facial cleanser |
| 30min | 27.31±1.97 | 23.15±1.65 | 33.54±2.25 |
| 1h | 27.55±2.18 | 23.19±2.51 | 35.44±3.65 |
| 7h | 28.63±3.31 | 26.89±2.64 | 32.19±2.56 |
The high viscosity moisturizing amino acid facial cleanser can protect and supplement skin barrier. Under a stable environment, the measured data shows that the water locking and moisturizing time is still higher than a blank value.
Example 8: testing of squalane-embedded high viscosity moisturizing amino acid facial cleanser
1. Squalane liposome was prepared according to the preparation method described in example 1, formulation H in example 3; sampling, selecting emulsified particles with different sizes by microscopic image control analysis under a high power microscope, and measuring the particle diameter by a three-point method, wherein the measured particle diameter is 20 nm-60 nm squalane liposome.
2. The facial cleanser was prepared according to the preparation method described in example 3, and the formula was formula D in example 3;
(1) The obtained facial cleanser is squalane-embedded high-viscosity moisturizing amino acid facial cleanser, and is subjected to viscosity test after standing and aging for 24 hours at room temperature;
NDJ-1 type rotary viscometer test conditions are selected: rotor No. 3, 6rpm;
74.5 (pointer reading) × 200 (coefficient) =14900mpa.s.
(2) And (3) performing foam test after the squalane-embedded high-viscosity moisturizing amino acid facial cleanser is stood and aged for 24 hours at room temperature, wherein the test method is measured by using a Roche foamer according to GB/17173:
and (3) testing mass concentration: 2 percent;
and (3) testing temperature: at 40 ℃;
the initial foam height was: 128 + -3 mm (3 measurements are averaged);
foam height after 10min 115. + -.3 mm (3 measurements mean).
(3) Spot pasting experiment: selecting 31 subjects, wherein the age of the subjects is 23-38 years old;
the number of sensitive muscles is required to be at least 50 percent of the total number (the number of sensitive muscle screening rolls is measured by 5 percent lactic acid solution), and the number of actual sensitive muscles is 17;
applying spots of the squalane-embedded high-viscosity moisturizing amino acid facial cleanser to the curved side of the forearm of a subject, lightly pressing with hands to uniformly apply the patches to the skin for 24 hours, removing the spots, and recording reaction results for 30min, 24 hours and 48 hours after the indentations disappear;
all the testers had negative reaction. Without weak erythema, edema, infiltration, pimple, etc.
(4) Moisture content of skin: under the test conditions of constant temperature and constant relative humidity (25 ℃, 35 ℃) of an organoleptic test laboratory, a skin moisture content test probe is used to select 10 human subjects with the ages of 25-38 years from a Cornemeter CM825 of Germany CK company (Courage + Khazaka company, germany) for testing, and the test results are shown in the following table 8;
TABLE 8 test results
| Time | Blank space | Commercial facial cleanser | High-viscosity moisturizing amino acid facial cleanser |
| 30min | 27.55±1.60 | 24.00±1.82 | 31.38±3.35 |
| 1h | 27.90±2.20 | 24.85±2.90 | 33.49±3.43 |
| 7h | 28.63±3.88 | 27.00±3.57 | 32.15±2.57 |
The high viscosity moisturizing amino acid facial cleanser can protect and supplement skin barrier. Under a stable environment, the measured data shows that the water locking and moisturizing time is still higher than a blank value.
As shown by comparing the test results of examples 5 to 8, the squalane-coated liposome microcapsules denatured at high and low temperatures prepared in example 1 have a significant advantage in both viscosity of the facial cleanser and moisturizing effect compared with the undenatured squalane liposome microcapsules prepared in example 2.
The amino acid facial cleanser mainly takes amino acid surfactants as main materials, has fine foams, moderate cleaning force, soft and mild skin feel when in use, has weak acidity in the whole formula, and is close to the pH value of healthy skin of a human body.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; such modifications and substitutions do not depart from the spirit and scope of the corresponding claims.
Claims (6)
1. A squalane-embedded high-viscosity moisturizing amino acid facial cleanser is characterized in that: the facial cleanser consists of the following components in parts by weight:
25-40 parts of glycerol;
5363 parts of butanediol 5~8;
8 to 14 parts of cocoyl potassium glycinate;
5363 parts of sodium cocoyl malate 2~6;
5-10 parts of alkyl glycoside;
cocamidopropyl betaine 5~8 parts;
5363 parts of cetostearyl alcohol 1~2;
1.5 to 4 parts of ethylene glycol stearate;
1.5 to 2 parts of citric acid;
0.5 to 1 part of glycerol stearate;
0.05 to 0.1 portion of ethylene diamine tetraacetic acid disodium;
1 part of vitamin E acetate;
0.5 part of p-hydroxyacetophenone;
0.5 to 1 part of collagen;
5363 parts of squalane liposome 4~8;
22.45 to 53.4 parts of deionized water;
the preparation method of the facial cleanser comprises the following steps:
(1) Adding the first part of the glycerol, the butanediol, the potassium cocoyl glycinate, the sodium cocoyl malic amino acid, the alkyl glycoside, the cocamidopropyl betaine, the cetostearyl alcohol, the ethylene glycol stearate, the glyceryl stearate, the disodium ethylene diamine tetraacetate, the vitamin E acetate, the p-hydroxyacetophenone and the deionized water with the above dosage, vacuumizing, heating and stirring for reaction to obtain a phase A;
(2) Adding citric acid into the second part of the deionized water, and stirring and dissolving to obtain a citric acid aqueous solution as a phase B;
(3) Adding collagen into the third part of the deionized water, and stirring and dissolving to obtain a phase C;
(4) Adding the phase B obtained in the step (2) into the phase A obtained in the step (1), heating and stirring, and cooling to obtain a phase D;
(5) Adding the phase C obtained in the step (3) into the phase D obtained in the step (4), keeping the temperature, stirring, cooling and obtaining a phase E;
(6) Adding the squalane liposome into the phase E obtained in the step (5), keeping the temperature and stirring, cooling, standing and aging to obtain the squalane-embedded high-viscosity moisturizing amino acid facial cleanser;
the weight of the first part of deionized water, the second part of deionized water and the third part of deionized water is 60 to 90 percent, 5 to 20 percent and 5 to 20 percent of the total weight of the deionized water respectively;
the squalane liposome is prepared by the method a or the method b:
method a, (a 1): after the emulsification kettle is cleaned and disinfected, adding 20 to 28 parts of squalane, 3~8 parts of caprylic acid/capric acid triglyceride and 5~6 parts of phytosterol into the emulsification kettle, heating, stirring, cooling and discharging to a raw material barrel;
(a2) The method comprises the following steps Placing the raw material barrel in the step (a 1) in a refrigerator for cooling and storing, taking out for heating and preserving, cooling and storing again, and keeping for later use after the period of 3~6 of cold-hot alternating circulation;
(a3) The method comprises the following steps After the emulsification kettle is cleaned and disinfected, adding 8 to 12 parts of deionized water, adding 10 to 15 parts of hydrogenated lecithin into the emulsification kettle, starting sealed stirring, introducing nitrogen and stirring;
(a4) The method comprises the following steps Adding the raw materials treated in the step (a 2) into the emulsifying kettle in the step (a 3), vacuumizing, stirring, heating and preserving heat; adding 3 parts of 1,2-hexanediol and deionized water, vacuumizing the emulsifying kettle, increasing the stirring speed, opening homogenizing and shearing for 8 to 12min, reducing the stirring speed, and cooling and discharging to obtain the squalane liposome;
or method b, (b 1): after the emulsification kettle is cleaned and disinfected, adding 8 to 12 parts of deionized water, adding 10 to 15 parts of hydrogenated lecithin into the emulsification kettle, starting sealed stirring, introducing nitrogen and stirring;
(b2) The method comprises the following steps Adding 20 to 28 parts of squalane, 3~8 parts of caprylic/capric triglyceride and 5~6 parts of phytosterol into an emulsifying kettle, vacuumizing, stirring, heating and preserving heat; adding 3 parts of 1,2-hexanediol and deionized water, increasing the stirring speed, opening the mixture to be homogenized and sheared for 8 to 12min, reducing the stirring speed, and discharging after cooling to obtain the squalane liposome;
the total amount of the deionized water in the steps (a 3) and (a 4) is 20 to 28 parts; the total amount of the deionized water in the steps (b 1) and (b 2) is 20 to 28 parts.
2. The squalane-embedded high-viscosity moisturizing amino acid facial cleanser according to claim 1, wherein the reaction temperature in the step (1) is 71-80 ℃, and the stirring speed is 300-500rpm.
3. The squalane-embedded high-viscosity moisturizing amino acid facial cleanser according to claim 1, wherein the temperature of the step (4) is 76 to 85 ℃, and the temperature of the step (4) is 56 to 65 ℃; the stirring speed is 300 to 500rpm.
4. The squalane-embedded high-viscosity moisturizing amino acid facial cleanser according to claim 1, wherein the cooling temperature in the step (5) is 36-45 ℃.
5. The squalane-embedded high-viscosity moisturizing amino acid facial cleanser according to claim 1, wherein the cooling rate in cooling in (4) and (5) is 0.5-1.5 ℃/min.
6. Use of the squalane-embedded high viscosity moisturizing amino acid facial cleanser of claim 1 in the preparation of cosmetics.
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